Water → 6-Chloro-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine] maleate

HRID 1660355노트

반응식

HRID 1660355 반응식
[Cl:1][C:2]1[CH:7]=[C:6]2[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[CH2:9][C:10]3([CH2:15][CH2:14][N:13](C#N)[CH2:12][CH2:11]3)[C:5]2=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[C:32]([OH:39])(=[O:38])/[CH:33]=[CH:34]\[C:35]([OH:37])=[O:36]>O1CCCC1.CCOCC>[C:32]([OH:39])(=[O:38])/[CH:33]=[CH:34]\[C:35]([OH:37])=[O:36].[Cl:1][C:2]1[CH:7]=[C:6]2[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[CH2:9][C:10]3([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[C:5]2=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 444266Maleic AcidHCID 131540506-Chloro-1'-cyano-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine]HCID 21226445Aluminium lithium hydride

생성물 1

HCID 128016246-Chloro-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine] maleate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 3.4 g of 6-chloro-1'-cyano-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine], Example 26, in 50 ml of tetrahydrofuran is added dropwise to a refluxing slurry of 1.0 g of lithium aluminum hydride in 50 ml of tetrahydrofuran. After total addition the mixture is stirred at reflux for 2.5 hours before being treated with water and alkali. The resulting oily product, in ether, is converted to its maleic acid salt which is recrystallized from an ethyl alcohol-ether mixture to provide off-white granules, mp 174.5°-175.5° C. of 6-chloro-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine] maleate.

후처리

  1. additionAfter total addition the mixture
  2. temperatureat reflux for 2.5 hours
  3. customis recrystallized from an ethyl alcohol-ether mixture

출처 및 근거

ORD 기록
ord-e84267c525ec4855823a08ca73216539
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04307235

반응 노트

불러오는 중…